Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethyl Sulfate → 1H-Purine-2,6-dione, 3,7-dihydro-8-(2-(1,1'-biphenyl)-4-ylethenyl)-1,3-diethyl-7-methyl-, (E)-
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethyl Sulfate | HCID 6497 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 1H-Purine-2,6-dione, 3,7-dihydro-8-(2-(1,1'-biphenyl)-4-ylethenyl)-1,3-diethyl-, (E)- | HCID 6448939 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 1H-Purine-2,6-dione, 3,7-dihydro-8-(2-(1,1'-biphenyl)-4-ylethenyl)-1,3-diethyl-7-methyl-, (E)- | HCID 6448940 | 30.8% |
반응 단계
Compound 163 (1.50 g, 3.89 mmol) obtained in Reference Example 104 was suspended in a mixed solvent of 13 ml of water, 3.9 ml of a 2N aqueous solution of sodium hydroxide, and 7 ml of methanol. To the suspension was dropwise added 0.55 ml (5.83 mmol) of dimethyl sulfate, and the resultant mixture was stirred at 60° C. for 4 hours. Water (10 ml) was added thereto, and the deposited crystals were collected by filtration and dried. The obtained crude crystals were purified by silica gel column chromatography, followed by recrystallization from ethyl acetate to give 480 mg (yield 28%) of Compound 164 as yellow columns.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05587378 |
| 출처 데이터셋 | uspto-grants-1996_12 |
| ORD ID | ord-671f35c06e53455f928e3a5ec289d8b4 |
| 출처 메모 | uspto-grants-1996_12 |